Multivariate statistical real-time monitoring of an industrial fed-batch process for the production of specialty chemicals

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Abstract

A large number of production processes for the manufacturing of specialty chemicals, pharmaceuticals, foodstuff, and materials for microelectronics are run in batch mode. Batch processes are “simple” in terms of equipment and operation design, but are often quite complicated in terms of product quality monitoring and of production scheduling and organization. In this paper an industrial case study is presented where the challenges related to the real-time estimation of the required time to manufacture a resin and to the instantaneous product quality estimation are addressed using multivariate statistical techniques. The industrial process is poorly automated, subject to several disturbances, and the batches have uneven lengths. It is shown that stage and batch lengths can be estimated in real time with an average error that is not larger than 20% of the inherent batch-to-batch variability, whereas quality estimations can be provided within the accuracy of the hardware instrumentation, but 240 times faster. The industrial benefits deriving from the use of the proposed monitoring system have been a drastic reduction of the number of samples that need to be analyzed by the lab, prompter adjustment of the processing recipe with consequent reduction of the total processing time, and improved capability to plan the production.

Introduction

Specialty chemicals (e.g. coatings, detergents, resins, adhesives, pigments, additives) are typically obtained by batch or semi-batch processing, where a “recipe” is used to coordinate a sequence of elementary operations (e.g. charge, mix, heat up, react, separate, cool down, discharge), which may be repeated several times during a batch.

Much is reported in the literature on the multivariate statistical monitoring of batch processes in the sense of detection of anomalous or faulty conditions by the analysis of process variables trends (Nomikos and MacGregor, 1994, Kosanovich et al., 1996, Neogi and Schlags, 1998, García-Muñoz et al., 2003, Kourti, 2003, Gunther et al., 2007). Information of this kind is extremely valuable to improve process understanding; however, in most cases it can be used only after the completion of the batch, regardless of the fact it has been obtained in real-time or from a retrospective analysis of the batch itself. For example, if a change in the quality of feeds is diagnosed on-line, the supplier would be interviewed before the next batch is started; if an incipient fouling of a heat exchanger is detected, maintenance would be started at the end of the batch; if the end-point quality of the product is anticipated to be out of specification, the product would not be delivered to the customer, and the reasons for this faulty batch would possibly be analyzed by interrogating the monitoring model. Much less attention has been directed towards the development of monitoring strategies able to provide some kind of information that can be used directly within the same batch from which this information is obtained. In this context, two typical challenges that need to be addressed by a monitoring system in the production of specialty chemicals are the real time estimation of the length of the batch (or the length of any production stage within the batch), and the real time estimation of the instantaneous quality of the product.

There are several specialty productions for which the total batch length is not known a priori, nor is it the length of any processing stage within the batch. Knowing in advance the processing time is useful for several reasons. In fed-batch processes, for example, new fresh material is charged into the process vessels at a convenient time instant. The ability to estimate in real time this instant (which may change from batch to batch) can result in savings both in the number of quality measurements to be processed by the laboratory and in the required total processing time (Marjanovic et al., 2006). On a different perspective, real-time estimation of the total length of the batch can be very useful for production planning, scheduling of equipment use, as well as to coordinate the operating labor resources.

Real time knowledge of the instantaneous quality of the product is extremely important in the manufacturing of several specialties. In fact, if the instantaneous product quality is not found to track a specified trajectory, the processing recipe must be adjusted in real time (possibly several times during a batch), and the batch is kept running until the end-point quality meets the specification. However, in most cases the product quality is not measured in real time, and to contain the laboratory-related expenses (in terms of: need of dedicated personnel, consumption of chemicals, and use analysis equipment) only few product samples are taken during the course of a batch and sent to the lab for analysis. Even so, in a typical industrial scenario where several productions are run in parallel, as many as 15,000 samples may need to be taken and analyzed each year, which can add up to an important fraction of the total product cost. From an operation perspective, due to the scarce number of measurements available during a batch and to the time delay inherent to the analysis, significant drifts on the quality profiles may be experienced before any intervention can be done on the batch being run. The net result is that the recipe adjustments are delayed, the total length of the batch is increased, and the economic performance of the process is further penalized.

In this paper, an industrial case study is presented where the challenges related to the real time estimation of the required processing time and to the instantaneous product quality estimation are addressed using multivariate statistical techniques based on the projection onto latent structures (Wold et al., 2001). Reference is made to a fed-batch process where a resin is produced. It is shown that, by appropriately using existing techniques, information can be extracted from available process measurements that can significantly improve the overall performance of the process. Although the results presented are tailored to a specific case study, we nevertheless believe that the approach we have taken is quite general, and can be useful both to practitioners and to academics for successful design and implementation of data-based monitoring techniques.

Section snippets

The process and related challenges

A high molecular weight polyester resin is produced by catalytic poly-condensation of carboxylic acids and alcohols in an industrial facility where several different specialty chemicals are manufactured. The product quality is determined by the combined values of two indicators, namely the resin acidity number (NA) and the resin viscosity (μ). A schematic of the production process is shown in Fig. 1.

Two distinct production stages are present. Raw materials, catalyst and additives are initially

Projection to latent structures

In order to design the monitoring models, a multivariate statistical technique is used, namely projection to latent structures (PLS), also known as partial least squares regression (Geladi and Kowalski, 1986, Kourti and MacGregor, 1995, Wise and Gallagher, 1996). PLS is a regression technique that allows one to deal with correlated process variable measurements (e.g. temperatures, pressures, flow rates, …) and to relate them to response variables (e.g. quality or time).

Let us first consider a

Stage 1 monitoring: estimation of the stage length

The number of quality measurements within this stage is too small to allow designing a PLS model for the real-time estimation of the product quality. Therefore, to monitor the evolution of the batch, the stage length τ was estimated instead. The possibility of knowing the value of τ in advance would allow the operators to further reduce the number of samples that need taking for analysis, because samples would only be taken starting from the time when the stage is expected to terminate. Thus,

Stage 2 monitoring

During Stage 2 the pre-polymer is transformed into the end product. Interventions on the recipe are carried out by the operators during this stage in response to the quality measurements coming from the lab.

To monitor this production stage two tools were designed: a soft sensor estimating in real time the product quality from process measurements, and a soft sensor estimating in real time the total length of the stage.

Conclusions

In this paper it was shown through an industrial case study how, by considering a blend of engineering judgment and mathematical modeling, multivariate statistical techniques can be exploited to assist the real-time monitoring of product quality and to deliver helpful information for an effective production planning in the semi-batch processing of specialty chemicals.

An evolving PLS modeling approach was exploited for the estimation of the duration of the batch. Namely, it was shown that, by

Acknowledgements

Partial financial support to this work was provided by the University of Padova within Progetto di Ateneo 2005 “Image analysis and advanced modelling techniques for product quality control in the process industry”.

PF, FB and MB would like to thank Sirca S.p.A. for allowing them to publish their industrial data.

References (22)

  • S. Beaver et al.

    Cluster analysis for autocorrelated and cyclic chemical process data

    Ind. Eng. Chem. Res.

    (2007)
  • Cited by (25)

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